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投稿时间:2021-04-13 修订日期:2021-11-17
投稿时间:2021-04-13 修订日期:2021-11-17
中文摘要: 本文利用以水作载流的氢化物发生-原子荧光光谱仪测定了以磷块岩为原料自制的磷酸中的砷(As)。利用硫酸法溶融磷块岩自制出磷酸,优化仪器的工作条件,通过条件实验选择出适用于测定砷所需的盐酸和5% L(+)-抗坏血酸-5% 硫脲的用量。原子荧光光谱法测定结果如下:在0.5 ng·mL-1 ~ 8.0 ng·mL-1浓度范围内线性相关系数R2=0.99996;检出限为0.0018 ng·mL-1,样品的相对标准偏差(RSD)为0.82 %,样品的加标回收率在92.4 % ~ 103.4 %。通过与电感耦合等离子体发射光谱法(ICP-OES)比对,结果一致。
中文关键词: 磷块岩,磷酸,原子荧光,砷
Abstract:In this paper, the content of arsenic in phosphoric acid prepared from phosphorite was determined by a hydride generation-atomic fluorescence spectrometer with water as the carrier. Phosphoric acid was produced by melting the phosphorous rock by the sulfuric acid method, the working conditions of the instrument were optimized, and the amount of hydrochloric acid and 5% L(+)-ascorbic acid-5% thiourea suitable for the determination of arsenic was selected through the condition experiment. The results of atomic fluorescence spectrometry are as follows: the linear correlation coefficient R2 is 0.99996 in the concentration range of 0.5 ng · ml-1 ~ 8.0 ng · ml-1; the detection limit is 0.0018ng ·ive standard deviation (RSD) is 0.82%; the recoveries of samples are 92.4% ~ 103.4%. Compared with inductively coupled plasma emission spectroscopy (ICP-OES), the results are consistent.
文章编号: 中图分类号:O657.3 文献标志码:
基金项目:核能开发项目(测HDJS2102)
引用文本:
王娅楠,郭冬发,李黎,李伯平,张良圣,刘瑞萍.原子荧光光谱法测定以磷块岩为原料制备磷酸中的砷[J].中国无机分析化学,2021,11(6):8-11.
WANG Yanan,GUO Dongfa,LI Li,LI Boping,ZHANG Liangsheng,LIU Ruiping.Determination of arsenic inphosphoric acid prepared from phosphorite by atomic fluorescence spectrometry[J].Chinese Journal of Inorganic Analytical Chemistry,2021,11(6):8-11.
王娅楠,郭冬发,李黎,李伯平,张良圣,刘瑞萍.原子荧光光谱法测定以磷块岩为原料制备磷酸中的砷[J].中国无机分析化学,2021,11(6):8-11.
WANG Yanan,GUO Dongfa,LI Li,LI Boping,ZHANG Liangsheng,LIU Ruiping.Determination of arsenic inphosphoric acid prepared from phosphorite by atomic fluorescence spectrometry[J].Chinese Journal of Inorganic Analytical Chemistry,2021,11(6):8-11.